US5382219A - Ultra-light composite centrifuge rotor - Google Patents

Ultra-light composite centrifuge rotor Download PDF

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Publication number
US5382219A
US5382219A US08/202,676 US20267694A US5382219A US 5382219 A US5382219 A US 5382219A US 20267694 A US20267694 A US 20267694A US 5382219 A US5382219 A US 5382219A
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US
United States
Prior art keywords
rotor
rotor plate
tube
centrifuge
axis
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
US08/202,676
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English (en)
Inventor
Mohammad G. Malekmadani
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Composite Rotor Inc
Original Assignee
Composite Rotor Inc
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Composite Rotor Inc filed Critical Composite Rotor Inc
Priority to US08/202,676 priority Critical patent/US5382219A/en
Application granted granted Critical
Priority to US08/373,544 priority patent/US5562582A/en
Publication of US5382219A publication Critical patent/US5382219A/en
Assigned to LRM HOLDINGS, INC. reassignment LRM HOLDINGS, INC. FORM UCC1 Assignors: COMPOSITE ROTOR, INC.
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04B—CENTRIFUGES
    • B04B5/00—Other centrifuges
    • B04B5/04—Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers
    • B04B5/0407—Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers for liquids contained in receptacles
    • B04B5/0414—Radial chamber apparatus for separating predominantly liquid mixtures, e.g. butyrometers for liquids contained in receptacles comprising test tubes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B04—CENTRIFUGAL APPARATUS OR MACHINES FOR CARRYING-OUT PHYSICAL OR CHEMICAL PROCESSES
    • B04B—CENTRIFUGES
    • B04B7/00—Elements of centrifuges
    • B04B7/08—Rotary bowls
    • B04B7/085—Rotary bowls fibre- or metal-reinforced
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T74/00—Machine element or mechanism
    • Y10T74/21—Elements
    • Y10T74/2109—Balancing for drum, e.g., washing machine or arm-type structure, etc., centrifuge, etc.

Definitions

  • This invention relates generally to centrifuge rotors, and relates more particularly to a rotor fabricated and reinforced with composite materials.
  • Centrifuges are commonly used in medical and biological research for separating and purifying materials of differing densities, such as viruses, bacteria, cells, protein, and other compositions.
  • a centrifuge includes a rotor typically capable of spinning at tens of thousands of revolutions per minute.
  • a preparative centrifuge rotor has some means for accepting tubes or bottles containing the samples to be centrifuged.
  • Preparative rotors are commonly classified according to the orientation of the sample tubes or bottles.
  • Vertical tube rotors carry the sample tubes or bottles in a vertical orientation, parallel to the vertical rotor axis.
  • Fixed-angle rotors carry the sample tubes or bottles at an angle inclined with respect to the rotor axis, with the bottoms of the sample tubes being inclined away from the rotor axis so that centrifugal force during centrifugation forces the sample toward the bottom of the sample tube or bottle.
  • Swinging bucket rotors have pivoting tube carriers that are upright when the rotor is stopped and that pivot the bottoms of the tubes outward under centrifugal force.
  • centrifuge rotors are fabricated from metal. Since weight is concern, titanium and aluminum are commonly used materials for metal centrifuge rotors.
  • Fiber-reinforced, composite structures have also been used for centrifuge rotors.
  • Composite centrifuge rotors are typically made from laminated layers of carbon fibers embedded in an epoxy resin matrix. The fibers are arranged in multiple layers extending in varying directions at right angles to the rotor axis. During fabrication of such a rotor, the carbon fibers and resin matrix are cured under high pressure and temperature to produce a very strong but lightweight rotor.
  • U.S. Pat. Nos. 4,781,669 and 4,790,808 are examples of this type of construction.
  • fiber-reinforced composite rotors are wrapped circumferentially with an additional fiber-reinforced composite layer to increase the hoop strength of the rotor. See, for example, U.S. Pat. Nos. 3,913,828 and 4,468,269.
  • Composite centrifuge rotors are stronger and lighter than equivalent metal rotors, being perhaps 60% lighter than titanium and 40% lighter than aluminum rotors of equivalent size.
  • the lighter weight of a composite rotor translates into a much smaller mass moment of inertia than that of a comparable metal rotor.
  • the smaller moment of inertia of a composite rotor reduces acceleration and deceleration times of a centrifugation process, thereby resulting in quicker centrifugation runs.
  • a composite rotor reduces the loads on the centrifugal drive unit as compared to an equivalent metal rotor, so that the motor driving the centrifuge will last longer.
  • Composite rotors also have the advantage of lower kinetic energy than metal rotors due to the smaller mass moment of inertia for the same rotational speed, which reduces centrifuge damage in case of rotor failure.
  • the materials used in composite rotors are resistent to corrosion against many solvents used in centrifugation.
  • several cell holes are machined or formed into the rotor at an angle of 5 to 45 degrees, typically, with respect to the rotor axis.
  • the cell holes receive the sample tubes or bottles containing the samples to be centrifuged.
  • Cell holes can be either through holes that extend through the bottom of the rotor, or blind holes that do not extend through the bottom. Through cell holes are easier to machine than blind cell holes, but require the use of sample tube holders inserted into the cell holes to receive and support the sample tubes.
  • the present invention provides a centrifuge rotor having a composite rotor plate, composite tube holders, composite bottom and top covers, and a hub to attach the rotor plate to a centrifuge.
  • the rotor plate has counterbored through holes with each counterbore defining an annular step. The holes are equally spaced in an annular array adjacent to the plate periphery.
  • the tube holders are cylindrical in shape and are mounted to the rotor plate in each of the counterbored through holes.
  • Each tube holder has an circumferential flange that mates with and is bonded to the annular step in a counterbore of the rotor plate.
  • Each tube holder has an open top for receiving a sample tube and a closed bottom for supporting the sample tube.
  • the bottom cover is an axi-symmetrical shell structure that mounts on the rotor plate and covers the bottoms of the tube holders.
  • the present invention uses only composite materials in a hollow structure and thus has the advantages of ultra-light weight, Low energy, and corrosion resistance.
  • FIG. 1 is a perspective view of a fixed-angle centrifuge rotor according to the present invention. Bottom and top covers are hoe shown.
  • FIG. 2 is a sectional view of the centrifuge rotor of FIG. 1.
  • FIG. 3 is a sectional view of a filament-wound tube holder during a preliminary stage in its fabrication.
  • FIG. 4 is a sectional view of the filament-wound tube holder.
  • FIG. 5 is a perspective view of the filament-wound tube holder of FIG. 3 and equipment used in its fabrication.
  • FIG. 6 is a section view of a rotor plate of the centrifuge rotor of FIG. 1.
  • FIG. 7 is a sectional view of a fixed-angle centrifuge rotor of the present invention illustrating another embodiment of the invention, which orients the radially-outer portions of the rotor plate at an angle to the rotor axis.
  • FIG. 8 is a sectional view of a centrifuge having vertically oriented tube holders.
  • FIG. 9 is a perspective view of the filament-wound tube holder of FIG. 3.
  • FIGS. 1 through 9 of the drawings depict various preferred embodiments of the present invention for purposes of illustration only.
  • One skilled in the art will readily recognize from the following discussion that alternative embodiments of the structures and methods illustrated herein may be employed without departing from the principles of the invention described herein.
  • the preferred embodiment of the present invention is a fixed-angle centrifuge rotor 10 fabricated from fiber-reinforced composite materials, as shown in FIGS. 1 and 2.
  • the rotor 210 has a rotor plate 12 composed of multiple layers 11 of resin-coated carbon fibers which are indexed to a predetermined repeating angle.
  • the fiber layers of the rotor plate 12 are oriented at right angles to the axis of rotation 14 of the rotor 10 to provide the optimum strength against centrifugal forces generated when the rotor is rotating.
  • the rotor 10 includes a hub 16 that mounts to a spindle 17 (FIG. 2) of a centrifuge machine (not shown), which spins the rotor about its axis 14.
  • the rotor plate 12 has six counterbored through holes 18, each angled toward the rotor axis 14 and each containing a tube holder 20.
  • Each counterbored hole 18 has an annular step 22 (FIG. 2) that supports a circumferential flange 24 on the tube holder 20.
  • the radially outer surface 26 of the rotor plate 12 is conical in shape.
  • the rotor plate 12 includes six tube holders 20, each oriented with its axis 28 intersecting the rotor axis 14 at an oblique angle 30. All of the tube holders are preferably oriented at the same oblique angle with respect to the rotor axis, although this is not necessary. For symmetry, however, it is preferred that opposite tube holders be oriented at the same oblique angle.
  • Each tube holder 20 receives a sample tube or bottle (not shown) containing the materials to be centrifuged.
  • the rotor 10 need not have six tube holders, but it should have an even number of tube holders symmetrically arranged in an annular pattern.
  • FIG. 2 shows that the rotor 10 has a top axi-symmetric cover 32 and a bottom axi-symmetric cover 34, both to reduce the aerodynamic drag of the rotor 10.
  • the bottom cover 34 covers the lower portions of the tube holders 20 that protrude below the bottom of the rotor plate 12.
  • the bottom cover 34 is preferably bonded to an inner bottom surface 36 of the rotor plate 12 and to an outer edge 38 of the rotor plate.
  • the top cover 32 is removable, and covers the upper portions of the tube holders 20 that protrude above the top of the rotor plate 12.
  • the top cover 32 is screwed to spindle 17 of the centrifuge by a bolt 33.
  • the top and bottom covers are preferably fabricated from a carbon fiber-reinforced composite material.
  • the center of gravity of the tube holder 20 is positioned between the upper and lower surfaces of the rotor plate 12 so that the centrifugal loading of the tube holder on the rotor plate is in the plane of the rotor plate.
  • the thickness of the rotor plate 12 is about one-third of the height of the tube holder 20, and about one-third of the tube holder protrudes below the rotor plate and a similar amount protrudes above tile rotor plate.
  • FIGS. 3, 4, 5, and 9 illustrate the tube holder 20 utilized in the composite rotor 10.
  • FIGS. 3 and 9 show the tube holder 20 after filament winding by the apparatus of FIG. 5.
  • FIG. 4 shows the tube holder 20 after machining prior to insertion into the rotor plate 12.
  • the tube holders 20 are fabricated by helically and circumferentially winding a continuous carbon filament dipped in resin over a cylindrical mandrel 40 (FIG. 5).
  • the winding begins with a inner circumferential layer 42 (FIG. 3) wound onto the cylindrical mandrel 40.
  • the inner circumferential layer is increased in thickness at 44 to create a larger diameter.
  • a helical layer 46 of filament is wound onto the mandrel on top of the inner circumferential layer 42 and at the ends of the mandrel.
  • the helical layer 46 reinforces the entire tube holder 20 along its axis 28.
  • the fibers are oriented at an angle 50 with respect to the axis 28.
  • the angled portion 48 of the helical winding places the fibers partially transverse to the axis in area where the flange seat 24 will be machined.
  • the tube holder 20 is thus reinforced in the in-plane shear direction at the flange area where a downward centrifugal load acts on it.
  • An outer circumferential winding layer 52 is placed over the helical winding layer 46.
  • the outer layer 52 has a uniform thickness except for an increased thickness area 54 at the flange location in the midsection.
  • the wound shell is cured and cut into two halves no obtain two filament wound tube holders 20.
  • the outside of the tube holder is machined to form the flange 24, as shown in FIG. 4.
  • the flanged tube holders are bonded to the counterbored through holes 18 of the laminated rotor plate 12 with a structural adhesive such as epoxy.
  • the tube holders 20 are fabricated by circumferentially and helically winding a continuous filament of fibers coated with resin over the cylindrical mandrel 40.
  • the apparatus illustrated in FIG. 5 is used to dip a carbon fiber filament 56 into resin and wind the carbon filament onto the outside of the mandrel 40.
  • the mandrel 40 is rotated on a spindle 58.
  • the filament 56 is wound onto the mandrel 40 in either a circumferential or helical pattern.
  • the filament 56 is supplied by a spool 60 and is dipped in a resin bath 62.
  • a computer controlled bobbin 64 moves in two orthogonal directions and guides the filament onto the surface of the rotating mandrel 40.
  • the rotor plate 12 is fabricated by laminating several layers of unidirectional-carbon-fiber/epoxy-prepregnated tape oriented at right angles to the rotor axis.
  • the tape is made of longitudinally continuous fiber and coated with epoxy resin.
  • a typical tape is about 0.010 inch thick and contains about 65% fiber and 35% resin by weight.
  • the tape is cut, indexed to a predetermined repeating angle, and stacked to the height of the rotor plate.
  • the stack is then placed in a mold and cured under pressure at elevated temperatures to obtain a solid billet.
  • the billet is machined to the shape of a rotor plate 12 with an axis 14 at right angles to the plane of the tape layers.
  • An axial hole 66 is bored and threaded to receive the hub 16, and the through holes 18 are counterbored to form the annular step 22.
  • FIG. 7 An alternative rotor 100 of the present invention is illustrated in FIG. 7 in which a rotor plate 102 is formed into a conical section at an angle 103 that matches the angle 104 between the axis 108 of the tube holders and the rotor axis 109.
  • the fibers in rotor plate 102 are parallel to the upper and lower surfaces of the rotor plate.
  • the rotor plate is fabricated as described above with several laminated layers of fibers, but during curing the layers are formed into the conical shape. After curing, through holes 110 are counterbored into the rotor plate 102 and the tube holders 106 are bonded in place. Top and bottom covers 112 and 114 are added.
  • conical rotor plate 102 over the flat rotor plate 12 is that the conical plate can be thinner and still accommodate the angled counterbore. This reduces the weight and inertia of the rotor.
  • the invention disclosed herein provides a novel and advantageous centrifuge rotor fabricated from fiber-reinforced composite material.
  • the foregoing discussion discloses and describes merely exemplary embodiments of the present invention.
  • the invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof.
  • the tube holders 20 can be oriented with their axes 28 parallel to the rotor axis 14 to form a vertical tube rotor, as illustrated in FIG. 8.

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US08/202,676 1993-01-14 1994-02-25 Ultra-light composite centrifuge rotor Expired - Fee Related US5382219A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US08/202,676 US5382219A (en) 1993-01-14 1994-02-25 Ultra-light composite centrifuge rotor
US08/373,544 US5562582A (en) 1993-01-14 1995-01-17 Ultra-light composite centrifuge rotor

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US468493A 1993-01-14 1993-01-14
US08/202,676 US5382219A (en) 1993-01-14 1994-02-25 Ultra-light composite centrifuge rotor

Related Parent Applications (1)

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US468493A Continuation 1993-01-14 1993-01-14

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Application Number Title Priority Date Filing Date
US08/373,544 Continuation US5562582A (en) 1993-01-14 1995-01-17 Ultra-light composite centrifuge rotor

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US08/373,544 Expired - Fee Related US5562582A (en) 1993-01-14 1995-01-17 Ultra-light composite centrifuge rotor

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US (2) US5382219A (de)
EP (1) EP0678058B1 (de)
JP (1) JP2902116B2 (de)
KR (1) KR960700102A (de)
AU (1) AU5994794A (de)
DE (1) DE69417396T2 (de)
WO (1) WO1994015714A1 (de)

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US5477092A (en) * 1992-09-07 1995-12-19 British Nuclear Fuels Plc Rotor
WO1996035156A1 (en) * 1995-05-01 1996-11-07 Piramoon Technologies, Inc. Compression molded composite material fixed angle rotor
US5643168A (en) * 1995-05-01 1997-07-01 Piramoon Technologies, Inc. Compression molded composite material fixed angle rotor
US5667755A (en) * 1995-05-10 1997-09-16 Beckman Instruments, Inc. Hybrid composite centrifuge container with interweaving fiber windings
US5728038A (en) * 1997-04-25 1998-03-17 Beckman Instruments, Inc. Centrifuge rotor having structural stress relief
US5876322A (en) * 1997-02-03 1999-03-02 Piramoon; Alireza Helically woven composite rotor
US5972264A (en) * 1997-06-06 1999-10-26 Composite Rotor, Inc. Resin transfer molding of a centrifuge rotor
US6056910A (en) * 1995-05-01 2000-05-02 Piramoon Technologies, Inc. Process for making a net shaped composite material fixed angle centrifuge rotor
US6710498B1 (en) 1999-11-10 2004-03-23 Korea Advanced Institute Of Science And Technology Polymer composite squirrel cage rotor with high magnetic permeability filler for induction motor and method of making it
US6770244B2 (en) * 2001-05-03 2004-08-03 Hitachi Chemical Diagnostic, Inc. Dianostic sample tube including anti-rotation apparatus
US20050235481A1 (en) * 2001-03-24 2005-10-27 Lg Electronics Inc. Mover assembly of reciprocating motor
DE102004038706B4 (de) * 2004-03-02 2007-12-20 East-4D Gmbh Lightweight Structures Vorrichtung zur Herstellung von Faserverbundbauteilen, insbesondere schnelllaufender Rotoren, namentlich Zentrifugenrotoren
US20100184578A1 (en) * 2009-01-19 2010-07-22 Fiberlite Centrifuge, Llc Swing Bucket Centrifuge Rotor
US20100216622A1 (en) * 2009-02-24 2010-08-26 Fiberlite Centrifuge, Llc Fixed Angle Centrifuge Rotor With Helically Wound Reinforcement
US20100273626A1 (en) * 2009-04-24 2010-10-28 Fiberlite Centrifuge, Llc Centrifuge Rotor
US20100273629A1 (en) * 2009-04-24 2010-10-28 Fiberlite Centrifuge, Llc Swing Bucket For Use With A Centrifuge Rotor
US20110111942A1 (en) * 2009-11-11 2011-05-12 Fiberlite Centrifuge, Llc Fixed angle centrifuge rotor with tubular cavities and related methods
US20110136647A1 (en) * 2009-12-07 2011-06-09 Fiberlite Centrifuge, Llc Fiber-Reinforced Swing Bucket Centrifuge Rotor And Related Methods
US20130058187A1 (en) * 2011-09-06 2013-03-07 Brendan George Hart Agitation Apparatus with Interchangeable Module and Impact Protection Using Reactive Feedback Control
US20200306769A1 (en) * 2019-03-29 2020-10-01 Fiberlite Centrifuge Llc Fixed angle centrifuge rotor with tubular cavities and related methods
USD914236S1 (en) * 2018-03-19 2021-03-23 Fiberlite Centrifuge, Llc Centrifuge rotor

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US5732603A (en) * 1996-03-08 1998-03-31 Hughes Electronics Flywheel with expansion-matched, self-balancing hub
US6633106B1 (en) * 1999-09-30 2003-10-14 Dwight W. Swett Axial gap motor-generator for high speed operation
EP2302170A1 (de) * 2004-11-12 2011-03-30 Board of Trustees of Michigan State University Turbomaschine und Betriebsverfahren
DE102004062231B4 (de) * 2004-12-23 2012-12-13 Thermo Electron Led Gmbh Rotor für Laborzentrifugen
US7422554B2 (en) * 2005-08-10 2008-09-09 The Drucker Company, Inc. Centrifuge with aerodynamic rotor and bucket design
BR112012008216B1 (pt) 2009-10-06 2020-10-13 M-I L.L.C centrífuga de separação de lama de perfuração, método de substituição da porção cilíndrica da centrífuga de separação de lama de perfuração e método para separação de sólidos de fluidos de uma lama de perfuração
DE102009051207B4 (de) 2009-10-30 2013-10-17 Carbonic Gmbh Leichtbaurotor für Zentrifugen
KR101290930B1 (ko) 2011-06-21 2013-08-07 한양대학교 에리카산학협력단 우라늄 농축용 고속 회전 복합재 로터 및 그 제조 방법
KR101291617B1 (ko) * 2011-12-27 2013-08-01 한국기계연구원 관통형 복합재 보강물을 갖는 고정각 타입 하이브리드 원심분리기 로터
US10193430B2 (en) 2013-03-15 2019-01-29 Board Of Trustees Of Michigan State University Electromagnetic device having discrete wires

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WO1996035156A1 (en) * 1995-05-01 1996-11-07 Piramoon Technologies, Inc. Compression molded composite material fixed angle rotor
US5643168A (en) * 1995-05-01 1997-07-01 Piramoon Technologies, Inc. Compression molded composite material fixed angle rotor
US5776400A (en) * 1995-05-01 1998-07-07 Piramoon Technologies, Inc. Method for compression molding a composite material fixed angle rotor
US6056910A (en) * 1995-05-01 2000-05-02 Piramoon Technologies, Inc. Process for making a net shaped composite material fixed angle centrifuge rotor
US5667755A (en) * 1995-05-10 1997-09-16 Beckman Instruments, Inc. Hybrid composite centrifuge container with interweaving fiber windings
US5876322A (en) * 1997-02-03 1999-03-02 Piramoon; Alireza Helically woven composite rotor
US5728038A (en) * 1997-04-25 1998-03-17 Beckman Instruments, Inc. Centrifuge rotor having structural stress relief
WO1998048940A1 (en) * 1997-04-25 1998-11-05 Beckman Coulter, Inc. Centrifuge rotor having structural stress relief
US5972264A (en) * 1997-06-06 1999-10-26 Composite Rotor, Inc. Resin transfer molding of a centrifuge rotor
US6710498B1 (en) 1999-11-10 2004-03-23 Korea Advanced Institute Of Science And Technology Polymer composite squirrel cage rotor with high magnetic permeability filler for induction motor and method of making it
US20050235481A1 (en) * 2001-03-24 2005-10-27 Lg Electronics Inc. Mover assembly of reciprocating motor
US8049374B2 (en) * 2001-03-24 2011-11-01 Lg Electronics Inc. Mover assembly of reciprocating motor
US6770244B2 (en) * 2001-05-03 2004-08-03 Hitachi Chemical Diagnostic, Inc. Dianostic sample tube including anti-rotation apparatus
DE102004038706B4 (de) * 2004-03-02 2007-12-20 East-4D Gmbh Lightweight Structures Vorrichtung zur Herstellung von Faserverbundbauteilen, insbesondere schnelllaufender Rotoren, namentlich Zentrifugenrotoren
US20100184578A1 (en) * 2009-01-19 2010-07-22 Fiberlite Centrifuge, Llc Swing Bucket Centrifuge Rotor
US8282759B2 (en) * 2009-01-19 2012-10-09 Fiberlite Centrifuge, Llc Method of making a composite swing bucket centrifuge rotor
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US8147393B2 (en) 2009-01-19 2012-04-03 Fiberlite Centrifuge, Llc Composite centrifuge rotor
US8273202B2 (en) * 2009-02-24 2012-09-25 Fiberlite Centrifuge, Llc Method of making a fixed angle centrifuge rotor with helically wound reinforcement
US20120186731A1 (en) * 2009-02-24 2012-07-26 Fiberlite Centrifuge, Llc Fixed Angle Centrifuge Rotor With Helically Wound Reinforcement
US20100216622A1 (en) * 2009-02-24 2010-08-26 Fiberlite Centrifuge, Llc Fixed Angle Centrifuge Rotor With Helically Wound Reinforcement
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JPH08504672A (ja) 1996-05-21
US5562582A (en) 1996-10-08
WO1994015714A1 (en) 1994-07-21
DE69417396D1 (de) 1999-04-29
KR960700102A (ko) 1996-01-19
DE69417396T2 (de) 1999-09-16
EP0678058A1 (de) 1995-10-25
JP2902116B2 (ja) 1999-06-07
EP0678058A4 (de) 1995-09-01
EP0678058B1 (de) 1999-03-24
AU5994794A (en) 1994-08-15

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